Process for the production of alkali metal phytates



acid. Thereupon,

i atented Feb. 14, 1950 N l TED STAT ES PATENT OF I CE PnocEs-s role{run PRODUCTION or .ALKALI MET .PHYTAT Neal E. Artz, Oak Park, 111.,assignor to Corn Products ,R fin n ny, Ne York, .N- X, a corporation ofNew Jersey No Drawing. Application March 17, 1947, Serial No. 735,239

ration of alkali metal phytates directly from cal- :cium or magnesium:phytate or crude materials containing .the same.

Heretofore, sodium phytate, for example, has been prepared from metalphytates, such as cal- :cium :phytate, .by =first converting .thecalcium .phytate to iron phytate. is effected ,by dissolving thecal-ciumphytate in hydrochloric acid of proper concentration and addingto such solution, a solution of .ferric chloride in hydrochloric ironlphytate precipitates. The iron phytate, afiter being separated, is sspended in water and to this suspension is added :a solution -.of sodiumhydroxide, whereupon, Linsolubleierricrhydroxide is formed and remainsli n suspension :in'the alkaline solution. This is separated and the:sodium phytate is recovered Irom the filtrate by adding alcoholthereto. This causes the sodium .phytate to separate as .a-heavy .sirupin the bottom layer. ,If the wsirup iisseooled such complicated:procedure and by means :of my iinvention, alkali metal phytate may beprepared directly from calcium 'or magnesium iphytate or crude materialscontaining the same.

-The process oithepresent invention comprises reacting calcium phytateor magnesium ,phyta'te orcrude materials containing the same with asolution of alkali "metal hydroxide "at elevated "temperature andrecovering the alkali :metal Lphytate; :the .ratio of :phytate, which isa reactant, to alkali metal :hydroxide to water being within a specificrange.

Generally, the phytate and alkali :metal zhydroxide are mixed togetherand then sufiicient water isadded to produce :thedesired concentrationof :alkali metal :hydroxide in the -;resultant mixture.

" The 'heatifromwthe solution of the alkali :metal :hydroxide, is:generally suflicientto i-carry the reaction to'completionif 'thereac'tantsare mixed,

as above described, and 517116 temperature of the reactionimassusuallyattains =.a level :of about 220:F. t"240:-F. .Thezingredients;may be1=mixed :in .any order as long as there ,is sufficient heat@rovided when the phytate i re a se it t alkali metal hydrcxi solutionto complete the reaction. vIii-a solut on .of allgali :metal hydroxideis used, this must be hot when the tphytate is ad ed t ereto. Ir resta:is mixed w th a cold o u io o alka i meta h drox and the entire mixtureheat d rem-low i l vof al a i meta rhy at resu t; Isa d pend-ire u heconcentration of the hali metal ih droxide, alkali p osphat i obtained-It a solu ionef a k e a hyd oxi e i us d therrenar ien s sll met rh tse, i accordance i1 rresee invsntisn t t mperature of "shsolut s ish r bat lea tout 200 th :nh tate whic isea ta is added rthe to- Und -thessndi s h temp ratur o th ea ti nimss w a i t at ea t 230" F. Thetemperature of the reaction mass after the reaction has started shouldpreferably be maintained within the range of F. to 220 until the.reactiqn -i =complete. .If the tempera ure o th alkal met lh rQX-idsolution is ;much below @bQlz t 300 when the phytate is mixed therewibh(Qhe reaction does nottakeplace or ,proceeds tooi lowly :to-bepractical. Ilhe stem- =perature :of the reaction mass, irrespective ofthe means employed to initiate the reaction, may :exceed 220 1 withoutdetrimentally afiecting the reaction, but ,then there danger that the;-reactionwil1.=be diflicult to control.

The imetal -;phytat es which ,are satisfactory for the purposes of thepresent inventionare ,obtained. as precipitates ,trom .the treatment ofacidic plant extracts, gas f or example, corn steep quor-wi h ant. .,.ls eamat r a -a e ample, calcium hydroxide or lime; and magnesium hydr xiwhe corn s ep li uo 1 similar-acidic -;.eXtr-ac ts ,of plant ,materials,are neutralized with;9a1. ium hydroxide or lime or magnesiumahydrogide, gthe precipitates that form ,are .crude salts 'of phytic acidcomprising essentially calcium phittate or magnesium phytate orgmixtures thereof. If calcium- .hydr oxi de or .lime is used :-as aprecipitant, the precipitate consists mainlypf calcium phytate; but,since plant e r a ways contai ma nes um-s m Of this W111 be s ainsdi heci ita v ma nesium hydroxide is used as a precipitant, the precipitatecunsist rmem r ma ne um anhy e ybuta smallgamount of calcium may he,-contained therein.

While alkali metalrnh tates :may p pared satisfactorily, according to"th method of th m' e ti v ntion, from: m n s um ;-phy t hey m b -prarsd dram-m n sium iphrtat wmore satisfactorily according to the methodwhich forms the subject matter of copending application Serial No.735,240, filed March 17, 1947. Magnesium hydroxide, a product of thereaction between magnesium phytate and alkali metal hydroxide, asobtained at high temperatures used in the present invention is moredifficult to separate, as by filtration, from the alkali metal phytatein solution than magnesium hydroxide obtained at lower temperatures. 1

The amount of alkali metal hydroxide and the amount of water presentwhen the reaction is initiated may vary somewhat. If the amount ofphytate is kept constant, the amounts of alkali metal hydroxide andwater may vary as follows; For 5 parts of phytate, on a dry; basis, thealkali metal hydroxide, on a dry basis, should be at least 6 parts andmay range from 6 parts to 10 parts, and the amount of water should be atleast 2 parts and may range from 2 parts to parts. The preferred ratiowhen sodium hydroxide and calcium phytate are used, is 5 parts ofcalcium phytate to 8 parts of sodium hydroxide to 16 parts of water.

A considerable excess over the theoretical amount of alkali metalhydroxide should be used or the yield of alkali metal phytate is low. Onthe other hand, if too large an excess of alkali metal hydroxide isused, e. g., more than that specified above, no advantage is gained andthe alkali metal phytate is more difficult to purify.

As to the amount of water, there must be enough present to dissolve thealkali metal hydroxide and there must also be sufficient water presentto produce a somewhat fluid mixture, so that the reaction may proceeduniformly throughout the mixture. If too much water is used, thealkalinity of the solution is reduced to a point where the reaction doesnot go to completion.

After the ingredients are mixed together under proper conditions and thereaction is initiated, there should be allowed about 2 to 3 hours timefor the reaction to go to completion. During that time, the temperatureof the reaction mass should preferably be maintained at least at about190 F.

After the reaction has been completed, the mixture is allowed to cooluntil room temperature is reached. Water is then added to the reactionmixture which is in the form of a slurry. If not enough water is added,the slurry is too heavy to allow easy separation of the liquid phasefrom the solid phase and the alkali metal phytate may crystallize beforethe metal hydroxide, which precipitates as a result of the reactionbetween the phytate and alkali metal hydroxide, can be separated. On theother hand, if the solution is diluted too far, the reaction reversesitself and the resulting yield of alkali metal phytate is lower. Goodresults are obtained when the weight of the water added at this point isabout 6 times the weight of the phytate employed as one of thereactants. If the mixture is allowed to stand for more than 3 hoursafter reaching room temperature, there is danger that the alkali metalphytate therein will crystallize and then recovery of such phytate fromthe remaining mixture is diflicult to effect.

After the metal hydroxide has been separated from the slurry, as byfiltration, centrifugation, and the like, and the metal hydroxide cakehas been washed, alcohol is added to the clarified solution includingthe washings in amount, usually 10 percent to percent of its volume,sufficient to produce the maximal separation of alkali metal phytate asa sirup. The mixture is then allowed to stand. Within a short time, theliquid will separate into two layers-the heavy alkali metal phytatelayer being on the bottom. The upper layer is drawn off and saved forrecovery of alcohol and excess alkali metal hydroxide, both of which maybe reused in a subsequent reaction. The heavy alkali metal phytatelayer, which is sirupy in nature, may be used directly or it may bedried by passing over heated rolls or it may be allowed to crystallize,and the alkali phytate crystals recovered in conventional manner.

If it is desired to obtain the alkali metal phytate in its crystallineform rather than as a sirup, the specific gravity of the solution, afterremoval of metal hydroxide, may be adjusted to about 1.20 to 1.25 underwhich conditions alkali metal phytate may crystallize therefrom. Theaddition of not more than 10 percent of its volume of ethyl alcohol, forexample, to such a solution and stirring may cause separation of alarger crop of crystals of alkali metal phytate without causing theseparation of two liquid phases.

The alkali metal phytate thus obtained may contain some free alkalimetal hydroxide which changes to alkali metal carbonate on contact withair. If a product of greater purity is desired, the alkali metal phytatemay be redissolved in water, alcohol added thereto and the resultantmixture treated, as above described.

Among the alcohols which may be employed for recovering alkali metalphytate, in accordance with the present invention, are methyl alcohol,ethyl alcohol and isopropyl alcohol.

Any grade of reactants may be used, the commerical grades being quitesatisfactory.

Any equipment which is resistant to alkali and is provided with propermeans of heat control is suitable for purposes of the invention.

The following examples which are intended as informative and typicalonly and not in a limiting sense will further illustrate the invention,which is intended to be limited only in accordance with the scope of theappended claims.

Example 1.Commercial calcium phytate is prepared by adding lime to cornsteep liquor in amount to adjust the pH value thereof to 5.2. Theprecepitate which forms is separated, washed and dried in conventionalmanner. One hundred grams of such commercial calcium phytate is mixedwith 160 g. of flake sodium hydroxide in a beaker of one liter capacity.To this mixture is added slowly with stirring, during a 10 minuteinterval, 400 ml. of hot water. The mixture becomes quite hot, thetemperature ranging from 220 F. to 240 F., depending upon the rate atwhich water is added, and will boil over the sides of the beaker if thewater is added too rapidly.

After the water has been added, the mixture is allowed to stand untilthe temperature thereof reaches room temperature. The resulting slurryis then diluted to a volume of about 800 ml. with hot water, mixedcompletely and filtered or preferably centrifuged. To the clearfiltrate, containing sodium phytate in solution, about onefourth itsvolume of percent ethyl alcohol is added. The solution is completelymixed and allowed to stand. Within 15 to 30 minutes, the liquid willhave separated into two layersthe heavy sodium phytate layer being onthe bottom. The upper layer is drawn off and saved for recovery ofalcohol and excess alkali metal hydroxide. The sirup thus obtained maybe used directly, or it may be dried by means of heated .5 rolls to awhite flaky product of low moisture content, or it may bedried to theanhydrous condition and ground to a powder.

Example 2.-Twenty-five grams of commercial calcium phytate, prepared asdescribed in Examplel, is mixed with 40 g. of flake sodium hydroxide andthereto is added 100 m1. of hot water, the water being added a little ata time and with constant stirring. The mixture is kept hot, at atemperature of at least about 190 F., on the steam bath for 2 to 3hours.

One hundred and fifty milliliters of hot water is now added to thereaction mixture with thorough mixing and the suspension is centrifuged.The supernatant liquid is drawn off and a second, 200 ml. portion of hotwater is stirred up with the precipitate to recover the materialadhering to the precipitate. The suspension is centrifuged again and theliquid layer is drawn off into the same vessel that contains theoriginal supernatant liquor. To the combined solutions is added aboutone-fourth its volume or ethyl alcohol, and then the mixture is stirredcompletely and allowed to stand. After hour, the upper layer is drawnoff and the sirup remaining is dissolved in 100 ml. of hot water. Thirtyml. of alcohol is added to restratify the sirup, which is then used assuch or dried and ground to a powder. The sirup obtained here containsat least 80 percent of the total phytic acid phosphorus of the originalphytate as sodium phytate, as determined by the method of Heubner andStadler, Biochem. Z., 64, 422-37.

Example 3.Commercial magnesium phytate was prepared by adding magnesiumhydroxide to corn steep liquor in amount to adjust the pH value thereofto 6.5 The precipitate which formed was separated, washed, and dried inconventional manner. One hundred grams of such magnesium phytate wasmixed with 180 g. of flake sodium hydroxide and 300 ml. of hot water wasadded slowly to the mixture, which was constantly stirred. The heat ofsolution and reaction was suificient to raise the temperature of themixture to its boiling point. This mixture was more fluid than whencalcium phytate is treated in a like manner. After standing for 3 hours,300 ml. of water was added thereto and the solids were filtered off. Thefiltrate contained' 95 percent of the original phytic acid phosphorus,as determined by the aforementioned method, and when one-fourth the volume of the filtrate of ethyl alcohol was added, the typical sodiumphytate sirup formed.

Example 4.-To 25 grams of commercial calcium phytate, prepared accordingto Example 1, and 50 g. of potassium hydroxide, 50 ml. of hot water wasadded. The mixture became very hot and after standing for 2 hours, itwas diluted with 50 ml. of water and filtered and the cake was washed.To the combined filtrate and washings one-fourth volume of ethyl alcoholwas added, which caused a heavy sirupto settle out. The supernatantliquor was drawn off and the sirup layer was dried to a glassy materialthat was ground to a white, somewhat hygroscopic powder. This wasalkaline when dissolved, and when solutions of metal salts, such ascalcium chloride, were treated with the solution, typical insolublemetal phytates were formed.

Example 5 .Twenty-five liters of sodium phytate liquor, prepared inaccordance with the method described in Example 1, was clarified bycentrifugation. The specific gravity of the clarified liquor was 1.23.To the liquor was added 2.5 liters of ethyl alcohol. The entire liquidwas then stirred rapidly for 2 hours, during which time a jellylike massof sodium phytate crystals formed. The crystals were separated byfiltration, washed and air dried. The total weight of air dried crystalsof sodium phytate obtained was 5,580 gms.

I have, also, discovered that sodium phytate is effective in thetreatment of hard water. When small amounts of sodium phytate are addedto hard water, scale formation is prevented when such water is heated;corrosion by such water is inhibited; and the formation of agglomeratesof insoluble soaps is prevented when soap is added to such water. Whenlarger amounts or sodium phytate are added to hard water, the hardnessof such water may be completely obscured.

' When sodium phytate is added in low concentration to hard water, acloud is produced at first which increases as more sodium phytate isadded. When certain concentration of sodium phytate is attained, thecloud separates into a slight but discrete precipitate. Further addietion of sodium phytate causes the dispersal of the precipitate, thereappearance of the cloud and eventually the resolution and completedisappearance of the cloud, resulting in a clear S0111- tion.

The characteristics of water treated with sodi um phytate are altereddepending upon the amount of added sodium phytate.

Thus, when sodium phytate is added to hard water in low concentration,the tendency to deposit a scale of precipitated salts is reduced. Suchscale, when formed, interferes with heat transfer and reduces the amountof water-flow through the system.

I The following examples show the tendency of sodium phytate to preventincrustation due to calcium and magnesium salts in water.

Example 6.--Ordinary laboratory tap water (well water, Argo, Illinois)when boiled in an open flask began to cloud after boiling for abouthour, and by the end of 1 hour, the flask was coated with a tightlyadhering layer of precipitated salts. Three samples of the same water towhich sodium phytate, prepared in accordance with the present invention,had been added in concentrations of 10, 20 and 40 parts per million,respectively, were boiled in open flasks. These solutions becameslightly cloudy, the one containing the greatest quantity of sodiumphytate being most cloudy. On boiling for some time, the cloud increasedslightly but no material adhered to the flasks. Boiling was continuedfor 8 hours, during which time, as water boiled off, it was replacedwith fresh tap water. Although all solutions by this time contained somesuspended matter, this had not ad'- hered to the flasks. After standingovernight, the solutions were poured out and the flasks showed noincrustation. Thus, the material which separates on heating hard waterthat has been treated with sodium phytate can be flushed out of thesystem readily.

Example 7.-In another experiment, hard water (well water, Argo,Illinois) to which had been. added 250 parts per million of sodiumphytate, prepared in accordance with the present invention, was boiledunder reflux for 40 hours. The flocculent precipitate that formedremained in suspension throughout the boiling and poured out cleanly atthe end of the boiling period.

A sample-of the same hard water without sodium,

phytate, treated in the same manner, resulted in a flask heavilyencrusted with scale.

The next example demonstrates that water treated with sodium phytate ismuch less corrosive to iron than untreated water.

1 Example 8.-Iron nails placed in ordinary tap water (Well water, Argo,Illinois) showed definite corrosion in 1 hour. The same kind of nailsplaced in portions of the same water to which sodium phytate, preparedin accordance with the present invention, had been added inconcentrations of 25, 50, 100 and 200 parts per million showed norusting after 24 hours. After standing in the treated water for 1 week,the nails in the solution containing 200 parts per million of sodiumphytate showed no corrosion. Those that had stood in the phytatesolutions of lower concentration showed some rusting, the smaller theamount of sodium phytate employed, the greater the amount of corrosion.The nails in the untreated water were almost completely destroyed.

When sodium phytate is added to hard water in such concentration that adiscrete precipitate is formed, the treated water exhibits unusualbehavior upon the addition of soap. When titrated with soap solution bythe standard method of the American Public Health Association, hardwater, so treated, gives a slight but permanent lather when the amountof soap added is only that of the lather factor or a slightly greateramount. Although the water is not truly soft, it behaves in a mannersimilar to soft water. Further addition of soap does not result in theformation of curds of insoluble soap such as are produced when soap isadded to hard water. Instead, a fine and light floc forms which islargely retained in the slight lather and does not adhere to thecontaining vessel. Deposits of insoluble soaps formed by reaction ofsoluble soaps with the calcium and magnesium salts of hard water, adhereto and are difficult to remove from glassware, lavatories, bath tubs andlaundering equipment, whereas if the hard water has been treated firstwith sodium phytate, in an amount suflicient to form the slightprecipitate described above, insoluble soaps either do not adhere tosurfaces of contact or can be rinsed off easily.

The amount of sodium phytate necessary to produce the slight precipitatein hard water varies with the hardness of the particular water, but forWaters of ordinary hardness the requirement usually lies between 100 and300 parts per million. It is not necessary to know the hardness of thewater or the exact amount of sodium phytate to add in order to obtainthe desired precipitate, since if sodium phytate is placed in thecontainer to which hard water is to be added, the desired precipitate isformed as soon as sufficient calcium and/or magnesium have been added inthe form of the hard water. Once formed, the precipitate does notredissolve. Therefore, when soap is added, the precipitate exerts itsdispersing action on the insoluble soap which otherwise would form acurd.

Example 9.A 100 ml. portion of water, having a hardness of 200 parts permillion as calcium carbonate, was treated with 1.5 ml. of 2 percentsodium phytate solution, the sodium phytate being prepared in accordancewith the present invention. A distinct cloud formed, which soonseparated as a light, flocculent precipitate. To this suspension, 0.5ml. of standard soap solution (the lather factor for this soap solution)was added and the mixture was shaken vigorously. A light, but permanentlather formed. The solution was then diluted to 500 ml. with the014811131 hard water and the solution again was shaken. A light latherformed and remained. Addition of 20 ml. of the soap solution did notalter the characteristics of the solution. When it was poured out of theflask, no insoluble soap adhered to the containing flask. When 20 ml. ofthe soap solution was added to ml. of the untreated hard water, adefinite precipitate of insoluble soap formed. This settled out ofsolution and a large portion of the precipitate adhered tightly to theflask and could not be rinsed off.

Although water treated with sodium phytate in small quantities, asdescribed above, is not actually softened, hard water can be completelysoftened by the addition of sodium phytate. The amount of sodium phytaterequired depends upon the amount and kind of hardness of the particularwater.

The following example demonstrates the softening of hard water withsodium phytate.

Example 10.A 50 ml. sample of hard water that required 11.5 ml. of soapsolution for complete softening (in addition to the lather factor of 0.5m1.) corresponding to a hardness of 220 parts per million, was treatedwith 20 ml. of 2 percent sodium phytate solution, the sodium phytatebeing prepared in accordance with the present invention. When 0.5 ml. ofthe standard soap solution (the lather factor) was added to this sampleof treated water, a full permanent lather formed.

Water that has been softened by the addition of sodium phytate remainssoft after prolonged periods at the boiling temperature. This is nottrue of waters softened by sequestering agents, such as the sodiumpolyphosphates, as is demonstrated by the following example.

Example 11.Water containing 200 parts per million of hardness as calciumcarbonate, was treated with 4000 parts per million of sodium phytate,prepared in accordance with the present invention, the amount that hadbeen found necessary to completely soften this water. A like sample ofthe same water was treated with 2000 parts per million of sodiumhexametaphosphate,

' likewise the amount found necessary to completely soften the sample.Both the samples were boiled continuously under reflux and samples werewithdrawn at intervals for determination of hardness. After boiling for1 hour, 70 percent of the hardness had returned to the sample that hadbeen softened by sodium hexametaphosphate, and after being boiled 2 /2hours, the sample had returned to its original hardness. However, thesample that had been softened by addition of sodium phytate remainedcompletely soft 'after 48 hours at the boiling temperature.

One advantage of using sodium phytate for the purpose of preventingscale formation and of inhibiting the corrosive action of hard waterslies in the fact that this substance is much more stable to hydrolysisat boiling temperature or above than such substances as the sodiumpolyphosphates which are sometimes used for this purpose. Since thepolyphosphates are quickly destroyed at boiling temperature or above,they must be added continuously to the water. If sodium phytate is used,once the desired concentration is attained, its effectiveness isretained over long periods of time, even when evaporated water isreplaced by fresh, untreated water. The frequency of addition of thetreating agent is therefore reduced as well as the total amount oftreating agent required.

The following example demonstrates that sodium phytate is not onlystable at boiling temany type on new, scale free tubes.

' peratures but also that it is stable when a solution thereof is heatedunder pressure, to higher temperatures;

Example 1'2.Stand'ard hard water (250 parts per million calciumcarbonate hardness) softened with 1800 parts per million of sodiumphytate to 55 parts per million-calcium carbonate hardness,

- after being heated 2 weeks at 180 C. to 190 0.,

showed a reduction in apparent hardness to 14 parts per million calciumcarbonate hardness. The pH value of the solution-had dropped from toabout 8.

The same standard hard water (250 parts per million calcium carbonatehardness) softened with 1800parts per million of commercial-sodiumhexametaphosphate to 10 parts per million calcium carbonate hardness,increased to 2'7 parts per million calcium carbonate hardness whenheated for 4 hours at 180 C. and'to 185 parts per -million calcium.carbonate hardness after 19 /2 hours.- Water that had been softened tozero hardness by addition of 4000 parts permillion of sodium phytate.was subjected to a steam boiler test in a 10 pound steam boiler. After 6days operation and the addition of about 10 percent unsoitened water,the hardness increased to' '7 parts per million calcium carbonate.

The boiler test was discontinued after 48 days and examinations showedno scale formation of peared to. have been removed from the badly scaledcrown and shell. The hardness of the boiler solution had increased fromzero-to '7 parts per millioncalcium'carbonate hardness and. there was noappreciable increase in total solids.

Sodium phytate, prepared in accordance-with the present invention, maybe used in. the form of a sirup as recovered by alcohol, or it may beused in the form of a solution prepared by diluting such sirup to thedesired concentration. Likewise, the'sirup may be dried to a solid formof low moisture content and this solid may be used directly or solutionsof a desiredconcentration may be prepared from it. Crystallinesodium-phytate; obtained from its concentrated so lutions, likewise maybe used directly or in the form of solutions.

I claim:

1. The process which comprises effecting chemical reaction between (A) ametal phytate precipitate comprising essentially a material se lectedfrom the group consisting of calcium phytate, magnesium phytate. andmixtures thereof and obtained as a precipitate resulting from thetreatment of an acidic plant-extract with analkaline material selectedfrom the group consisting of lime. calcium hydroxide and magnesiumhydroxide, and (B) an alkali metal hydroxide in (C) a water medium, andrecovering alkali metal phytate; the ratio of said metal phytateprecipitate, on a dry basis, to alkali metal hydroxide, on a dry basis,to water being metal phytate precipitate 5, alkali metal hydroxide 6 to10 and water 2 to 20, the temperature of said medium during reactionbeing within the range of from about 190 F. to 240 F.

2. The process according to claim 1 wherein the temperature of saidmedium during reaction is maintained within the range of from about 190F. to 220 F. and the time during which the reaction is effected is about2 to 3 hours.

3. The process which comprises mixing (A) a dry metal phytateprecipitate comprising essentially a material selected from the groupconsisting of calcium phytate, magnesium phytate and Old scaleapmixtures thereof and obtained: as aprecipitate from the treatment ofan acidic plant extract withaan alkaline material selected from thegroup consisting of lime, calcium hydroxide and magnesium hydroxide with(B) a dry alkali metal hydroxide, adding water to-effect: a chemicalreaction between said metal phytate precipitate and said alkali metalhydroxide, and recovering alkali metalv phytate; the ratio of said metalphytate precipitate,- onadrybasis, to alkali metal hydroxide, 011a drybasis, to water being metal phytate precipitate 5, alkalimetal hydroxide6 to 10 andwater- 2-to 20, the temperature of said water during reactionbeing within-the range of from about 190 to 240 F.

e. .ihe process according to claim 3 wherein the temperatureof saidwater during reaction is maintained within. the range of from about 199F. to 220 and'the time during which the reaction is effected is about 2to 3 hours.

5. The process according to claim 4 wherein the alkali metal hydroxideis sodium hydroxide and-the alkali-metal phytate recovered is sodiumphytate.

6. The process. according to: claim. 4 wherein the alkali metalhydroxideis potassium hydroxide and the alkali metal phytate recovered ispotassium phytate.

'7. The process whichscomprises effecting chemical reaction between- (A)a metal phytate-precipitate comprising essentially a material selectedfrom the group consisting ofcalcium phytate, magnesium phytate andmixtures thereof and obtained as a precipitate resultingfrom thetreatment of an acidic plant extract with an alkaline material selectedfrom the group consisting of lime, calcium hydroxide, and ma nesiumhydroxide, and.- (B) an aqueous solution of an alkali metal hydroxide,and recovering alkali metal phytateg. the ratio. of' said metal phytateprecipitate, on a dry basis, to alkali metal hydroxide, on a drybasis,to water being metal phytate precipitate 5, alkali metal hydroxide6 tom. and. water 2 to 20,.the temperature of said aqueous solutionduring reaction being within the range of fromaboutl FLto 240 F 8.- Theprocess according to claim: 7 wherein the temperature ofsaid aqueoussolution during reaction is maintained within the range of from about190 F. to 220 F.

9. The process. whichcomprises effecting chemical reaction between (A) ametal phytate precipitatecomprising essentially. a material selectedfrom the group' consisting of calcium phytate, magnesium phytate andmixtures thereofandobtained asa precipitate resulting from the treatmentof an acidic plant extract with an alkaline material selected from thegroup consisting of line, calcium hydroxide and magnesium hydroxide, and(B) an alkali metal hydroxide in (C) a water medium, separating themetal hydroxide resulting from such reaction from the reaction mass, andtreating the liquor remaining from such separation with an alcoholselected from the group consisting of methyl alcohol, ethyl alcohol andisopropyl alcohol, whereby to recover the alkali metal phytate; theratio of said metal phytate precipitate, on a dry basis, to alkali metalhydroxide, on a dry basis, to water being metal phytate precipitate 5,alkali metal hydroxide 6 to 10 and water 2 to 20, the temperature ofsaid medium during reaction being within the range of from about 190 F.to 220 F.

10. The process which comprises mixing (A) a :dry metal phytateprecipitate comprising essenhydroxide, adding water to efiect a chemicalreaction between said metal phytate precipitate and said alkali metalhydroxide, separating the metal hydroxide resulting from such reactionfrom the reaction mass, and treating the liquor remaining from suchseparation with an alcohol selected from the group consisting of methylalcohol, ethyl alcohol and isopropyl alcohol, whereby to recover thealkali metal phytate; the ratio of said metal phytate precipitate, on adry basis, to alkali metal hydroxide, on a dry basis, to water beingmetal phytate precipitate 5, alkali metal hydroxide 6 to and water 2 to20, the temperature of said water during reaction being within the rangeof from about 190 F. to 220 F.

11. The process which comprises mixing (A) a dry metal phytateprecipitate comprising essentially a material selected from the groupconsisting of calcium phytate, magnesium phytate and mixtures thereofand obtained as a precipitate from the treatment of an acidic plantextract with an alkaline material selected from the group consisting oflime, calcium hydroxide and magnesium hydroxide with (B) a dry alkalimetal hydroxide, adding water to effect a chemical reaction between saidmetal phytate precipitate and said alkali metal hydroxide, diluting thereaction mass with water after said reaction is complete, separating themetal hydroxide resulting from such reaction from the reaction mass andrecovering alkali metal phytate from the liquor remaining after theremoval of said metal hydroxide; the ratio of said metal phytateprecipitate, on a dry basis, to alkali metal hydroxide, on a dry basis,to water for efiecting said reaction being metal phytate precipitate 5,alkali metal hydroxide 6 to 10 and water for reaction 2 to thetemperature of said water during said chemical reaction being within therange of from about 190 F. to 220 F.; and the amount of water added fordilution being such that the total amount of water present in thereaction mass after dilution does not exceed about ten times the weightof the metal phytate precipitate which is one of the reactants.

12. The process of producing sodium phytate which comprises mixing 5parts of a dry metal phytate precipitate comprising essentially calciumphytate and Obtained as a precipitate from the treatment of corn steepliquor with lime, with 8 parts of dry sodium hydroxide and adding 20parts of water to efiect the chemical reaction between said metalphytate precipitate and said sodium hydroxide, separating the calciumhydroxide formed and thereafter treating the remaining liquor with ethylalcohol to recover the sodium phytate; the temperature of said waterduring reaction being within the range of from about F. to 220 F. andthe amount of ethyl alcohol being about 25 percent of the volume of saidliquor.

13. The process of producing potassium phytate which comprises mixing 5parts of a dry metal phytate precipitate comprising essentially calciumphytate and obtained as a precipitate from the treatment of corn steepliquor with lime, with 10 parts of dry potassium hydroxide and adding 10parts of water to effect the chemical reaction between said metalphytate precipitate and said potassium hydroxide, separating the calciumhydroxide formed and thereafter treating the remaining liquor with ethylalcohol to recover the potassium phytate; the temperature of said waterduring reaction being within the range of from about 190 F. to 220 F.and the amount of ethyl alcohol being about 25 percent of the volume ofsaid liquor.

14. The process of producing sodium phytate which comprises mixing 5parts of a dry metal phytate precipitate comprising essentiallymagnesium phytate and obtained as a precipitate from the treatment ofcorn steep liquor with magnesium hydroxide, with 9 parts of dry sodiumhydroxide and adding 15 parts of water to effect a chemical reactionbetween said metal phytate precipitate and said sodium hydroxide,separating the magnesium hydroxide formed and thereafter treating theremaining liquor with ethyl alcohol to recover the sodium phytate; thetemperature of said water during reaction being within the range of fromabout 190 F. to 220 F. and the amount of ethyl alcohol being about 25percent of the volume of said liquor.

NEAL E. ARTZ.

REFERENCES CITED The following references are of record in the file ofthis patent:

UNITED STATES PATENTS Number Name Date 1,313,014 Posternak Aug. 12, 19191,644,246 Gams et a1 Oct. 4, 1927 2,318,663 Bird May 11, 1943 2,374,116Meincke, Jr Apr. 17, 1945

1. THE PROCESS WHICH COMPRISES EFFECTING CHEMICAL REACTION BETWEEN (A) AMETAL PHYTATE PRECIPITATE COMPRISING ESSENTIALLY A MATERIAL SELECTEDFROM THE GROUP CONSISTING OF CALCIUM PHYTATE, MAGNESIUM PHYTATE ANDMIXTURES THEREOF AND OBTAINED AS A PRECIPITATE RESULTING FROM THETREATMENT OF AN ACIDIC PLANT EXTRACT WITH AN ALKALINE MATERIAL SELECTEDFROM THE GROUP CONSISTING OF LIME, CALCIUM HYDROXIDE AND MAGNESIUMHYDROXIDE, AND (B) AN ALKALI METAL HYDROXIDE IN (C) A WATER MEDIUM, ANDRECOVERING ALKALI METAL PHYTATE; THE RATIO OF SAID METAL PHYTATEPRECIPITATE, ON A DRY BASIS, TO ALKALI METAL HYDROXIDE, ON A DRY BASIS,TO WATER BEING METAL PHYTATE PRECIPITATE 5, ALKALI METAL HYDROXIDE 6 TO10 AND WATER 2 TO 20, THE TEMPERATURE OF SAID MEDIUM DURING REACTIONBEING WITHIN THE RANGE OF FROM ABOUT 190*F. TO 240*F.